Methane → 3-(3-Phenylpropyl)aniline

HRID 1995477

반응식

HRID 1995477 반응식
[C:1]1([C:7](=O)[CH:8]=[CH:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([N+:16]([O-])=O)[CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.C.[H][H]>C(O)(=O)C.[Pd]>[C:1]1([CH2:7][CH2:8][CH2:9][C:10]2[CH:11]=[C:12]([CH:13]=[CH:14][CH:15]=2)[NH2:16])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

7

반응물 4

HCID 297MethaneHCID 1118Sulfuric AcidHCID 948623-NitrochalconeHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 4273073-(3-Phenylpropyl)aniline수율 71.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

253 g of 1-phenyl-3-(3'-nitrophenyl)-prop-2-en-1-one are suspended in 2.5 liters of glacial acetic acid. 196 g of concentrated sulfuric acid and 10 g of 10% strength Pd on animal charcoal are added and the mixture is hydrogenated under 1.1 bar hydrogen pressure, at 65°-70° C., until hydrogen is no longer absorbed. When the mixture has cooled, part of the acetic acid is distilled off, the residue is rendered alkaline with sodium hydroxide solution and extracted with ether, the organic phase is dried with sodium sulfate and filtered, the solvent is distilled off and the residue is then distilled. 150 g of 3-(3-phenylpropyl)-aniline, of boiling point 148° C./0.2 mbar, are obtained.

후처리

  1. customis no longer absorbed
  2. temperatureWhen the mixture has cooled
  3. distillationpart of the acetic acid is distilled off
  4. extractionextracted with ether
  5. dry with materialthe organic phase is dried with sodium sulfate
  6. filtrationfiltered
  7. distillationthe solvent is distilled off
  8. distillationthe residue is then distilled

출처 및 근거

ORD 기록
ord-ba290084dd3d4a58bcbfde730449839b
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04405358

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